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Dimethylformamide dimethyl acetal → 6-Dimethylaminomethylene-4,4-diphenylcyclohex-2-enone

HRID 1243853
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1243853
CO[CH:3](OC)[N:4]([CH3:6])[CH3:5].[C:9]1([C:15]2([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[CH2:20][CH2:19][C:18](=[O:21])[CH:17]=[CH:16]2)[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1>CN(C)C=O>[CH3:6][N:4]([CH:3]=[C:19]1[C:18](=[O:21])[CH:17]=[CH:16][C:15]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)([C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=2)[CH2:20]1)[CH3:5]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 78373Dimethylformamide dimethyl acetalHCID 1382802-Cyclohexen-1-one, 4,4-diphenyl-

Produkt 1

HCID 695944896-Dimethylaminomethylene-4,4-diphenylcyclohex-2-enoneAusbeute 56,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
20 °C

Versuchsvorschrift

4.77 g of N,N-dimethylformamide dimethyl acetal are added to a solution of 2.48 g of 4,4-diphenylcyclohex-2-enone in 20 Cm3 of N,N-dimethylformamide. The mixture is refluxed for about 4 hours. After cooling to a temperature in the region of 20° C., the solution is concentrated to dryness under reduced pressure (13 kPa). The residue is taken up in 50 cm3 of diisopropyl ether and allowed to precipitate for about 20 hours at a temperature in the region of 20° C. The solid is drained by suction, washed with three times 10 cm3 of diisopropyl ether and then dried under reduced pressure (13 kPa) over potassium hydroxide at a temperature in the region of 20° C. 1.7 g of 6-dimethylaminomethylene-4,4-diphenylcyclohex-2-enone are thus obtained in the form of a cream-coloured powder, the characteristics of which are as follows:

Aufarbeitung

  1. temperatureThe mixture is refluxed for about 4 hours
  2. concentrationthe solution is concentrated to dryness under reduced pressure (13 kPa)
  3. customto precipitate for about 20 hours at a temperature in the region of 20° C
  4. washwashed with three times 10 cm3 of diisopropyl ether
  5. dry with materialdried under reduced pressure (13 kPa) over potassium hydroxide at a temperature in the region of 20° C

Quellen und Nachweise

ORD-Eintrag
ord-f10d5c490f904ada9c2731611ed62f1a
Quelldatensatz
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07119115B2

Notizen zur Reaktion

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